Document Evr4Q2GYw53jpKK1mONw1JR6g
ARAA6_ 3304 :
486
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DuPont Haskell Laboratory Som for Health
#ha26_ 3304
To. Mrru rocker ain FROM: 1.C.Masanka
October 30, 2003
Quy Asstnce
E. Mylchreest
TEST SUBSTANCE STABILITY OF B24521
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MeHtasikcealllSRaempsleaNuPmrboejre:t Number:
HAAannsaakeyyliilccNllumTRebopeorrCtAoaNdut:mybierc:a Reference:
f224n521)
Dupe 13707
Notebook References:
[emus]
tachEed i athe anoalyrtest! rpeporot tno sattyprtoe equivrmnts For satis with F491 but
i
Company Senfized. Dossnatconteln TSCA CBI
TESTSUBSTANCE STABILITYOFH24921
HMasckelal SsamaplenNumbjere, unter
Analytical Report Number
[W24D001]
DuPont 13707
pAercseaamgepleofofHa-c2t4i9v21inwgraedrieenctei(v1e.d1)Juwliys1m1,ea2s0u0r3e,dn(d0 angyozned Jiayt1'4,s2r0a0n3. 1)
r
nominal for replicate analyses (n=3). The sponsorreported a purity
hen
to
le was submitted.
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ACKNOWLEGMENTS
Sample preparation by S. A. Riley (Chemisty Techniciand) sample analysis by
T. Ryan (Staff Chemist).
SIGNATURES
veponty: (R TnCeWa C.nMcatc siinnkte aes Senior Saft Chemis
20 ODtu-ezens
outs: 20: htaoc
--~
CompanySense.Does rtcartel rseacst
DuPont-13707 page 2o3f
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METHODS
Analysis of H-24921 was by high-performance liquid chromatography/tandem mass spectrometry(LEMS/MS). Negative-ion electrospray is used to generate negatively
charged ions i are selected with the firstMS quadrupole, collisionally
isgcated usingargon,and afragonimsmeonintorted. s used as an intemal standard.
`SAMPLE PREPARATION & ANALYSIS
wAaltieqruo(t1s0(00m.0L3)00t,o 0t.h0e3n0o1,miannadl 0c.o0n3c2en2tgrraatmiosn)sooffH3-0204,932011,wearned d3i2s2soplpvemd. iTn hNeasneopwuerree finutretrhnearldsiltuatneddartdoa0d.d0e03d1a5n,d0.a0n0a3l1y6z,edanacdc0o.r0d0i3n3g8toptphme wfiotlhlotwhiengapmpertohproida.te amount of
CHROMATOGRAPHIC CONDITIONS
LTpCnastrraummeentte:rs
Hewlett Packard Model 1100HPLC
Columa:
ZSoprmbax RX-C8, 2.1 mm x 150 mm,
FInljoewctRiaotne:Volume:
0s.o4umlL/min
~~
CCoolluummnn TSweimtpcehr:ature: ~~ 4300Cminutes
MobiGlreadPiheanste::
0.15% Acetic Acid/Acstonitrile
Time (min) % Acetonitrile
0009
55
6100
880
6710
55
MpSIansrtarummeentte:rs
Micromass Qualtro Micro Tandem MS
CTaopniilzaltairoynvomlotdaeg:e:
E2l7ec6tr0ospray (EST), negative ion
CSoounreceVoTleamgpeer:ature: 1250V0
-
SDeesaonlfvuantcitoinonT:emperature:
2,350" ipag
10.369 mz (danghter)
15 mz (parent) to 369 mlz
aughter)
Rinejteo ecnttiioonsn)Te. f]ric $2min(S04L
--~ Gompany Saniized. Does not contain TSCA CBI
DuPont-13707 page 3 of3
~~
CALIBRATION & QUANTITATION
A stock solution ofthe H-24921 (separate sample used as analytical reference) was `made in Nanopurewater. Appropriate aliquotsofthe stock were diluted withNanopure
STE=ioneeYccsi mbaotG iea,clE eCi eo otol nelsmvnee,se pShito y Nesaptw depv ioi eaavhiiorepeslsO sion epIndaeylerlheysfrsriee oeitsknisodocngvegrbpmi eendirkkvaeidrwoifiiesbompoNnfeiowopotnhmeedeid Analysisof H-24921 was by high-performance liquid chromatography/tandem mass
RESULTS
eHT:249or21 eluete$d f5roimathenHPLChceolumn as amreesonlveedppeeakvwiithsa reetnenotinon tnimee eg
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et. Tpeit etp Toa memstiseysiMeneer E1Noewe
TP R oms oo
arneteps e-- baete
bwiosd
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-----Otc sep on